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Preparation method of polymethoxymethylal

A technology of polymethoxymethylal and paraformaldehyde, which is applied in the preparation of organic compounds, chemical instruments and methods, molecular sieve catalysts, etc., can solve problems such as catalyst corrosion, and achieve improved coke capacity and high intracrystalline diffusion rate, activity-enhancing and stability-enhancing effects

Active Publication Date: 2013-05-29
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN101182367A and CN101962318A disclose the use of acidic ionic liquid as a catalyst, the method for preparing polyoxymethylene acetal by methanol and paraformaldehyde as raw materials, there is also the problem of serious corrosion of the catalyst
[0008] CN101665414A discloses a method of using acidic ionic liquid as a catalyst, using methylal and trioxane as raw materials to prepare polyoxymethylene formal, which also has the problem of severe catalyst corrosion
[0009] In summary, the catalysts used in the prior art have the disadvantage of being corrosive

Method used

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  • Preparation method of polymethoxymethylal
  • Preparation method of polymethoxymethylal
  • Preparation method of polymethoxymethylal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mix 40% silica sol, sodium metaaluminate, tetrapropylammonium bromide TPABr, sodium chloride, sodium hydroxide and water, stir for 20 minutes, put it into a reaction kettle, and crystallize dynamically at 170°C (200 rpm). 3 days. The crystallized product was quenched, filtered, washed with water until the pH value was 8, and dried at 120°C for 12 hours to obtain the original powder of ZSM-5 molecular sieve. The XRD spectrum is shown in figure 1 Middle curve 1, SEM photos see figure 2 , with an average grain diameter of 0.5 microns. The molar ratio of each raw material in the reaction mixture is: SiO 2 / Al 2 o 3 =76.90,H 2 O / SiO 2 =50.83, NaCl / SiO 2 =0.68, NaOH / SiO 2 =0.15, TPABr / SiO 2 = 0.40.

[0026] Treat the synthesized ZSM-5 molecular sieve raw powder with 0.3 mol / L acetic acid for 4 hours at 80°C for 3 consecutive times to obtain HZSM-5, then add boehmite, Tianqing powder and 0.3 mol / L nitric acid to mix, each The weight ratio of raw materials is ZSM-5 / ...

Embodiment 2

[0029] The ZSM-5 molecular sieve raw powder synthesized in [Example 1] was treated with 0.3 mol / liter hydrochloric acid at 80°C for 4 hours, continuously for 3 times, to obtain HZSM-5, and then added boehmite, Tianqing powder, 0.3 mol / liter Liter of nitric acid, HZSM-5 / Al 2 o 3 / Tian Qing powder = 1:1:0.1, extrusion molding, drying at 120°C for 12 hours, roasting at 550°C for 5 hours, pelletizing to obtain the catalyst.

[0030] The performance evaluation of the catalyst was carried out on a 300ml autoclave reaction device. Add 1.5 grams of catalyst, 80 grams of dimethyl ether, and 100 grams of paraformaldehyde in the autoclave, react for 4 hours at 110 ° C and make the pressure 4 MPa by filling nitrogen, filter and separate the catalyst and the reaction product, and analyze by gas chromatography to obtain The composition of the mixture is shown in Table 1.

Embodiment 3

[0032] According to the steps and conditions of [Example 1], only SiO in the synthetic formula 2 / Al 2 o 3 =40, 1,6-hexamethylenediamine was used as template agent, crystallized at 200°C for 5 days, and exchanged with 1.0 mol / L citric acid at 80°C for 10 hours. The average crystal grain diameter of the synthesized ZSM-5 molecular sieve raw powder is 1 micron.

[0033] The performance evaluation of the catalyst was carried out on a 300ml autoclave reaction device. Add 1.2 grams of catalyst, 50 grams of methanol, 50 grams of dimethyl ether, and 100 grams of paraformaldehyde in the autoclave, and react for 5 hours at 100 ° C and a pressure of 1 MPa by filling nitrogen, and filter and separate the catalyst and the reaction product. Chromatographic analysis, the composition of the obtained mixture is shown in Table 1.

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Abstract

The invention relates to a preparation method of polymethoxymethylal, mainly solving the problem that in the prior art, the catalyst has corrosivity. The method comprises the following step: by taking methanol or dimethyl ether and formaldehyde or trioxymethylene as raw materials, contacting the reaction raw materials with a catalyst to generate the polymethoxymethylal under the conditions that the molar ratio of the methanol or the dimethyl ether to the formaldehyde or the trioxymethylene is 1: (0.1-10), the reaction temperature is 50 to 200 DEGC and the reaction pressure of 0.1-10 MPa, wherein a molecular sieve ZSM-5 with the size of less than or equal to 5 microns is adopted as the active component of the used catalyst. through using the technical scheme, the problem is solved well. The method provided by the invention can be applied to industrial production of the poly methoxy methylal.

Description

technical field [0001] The invention relates to a preparation method of polymethoxy formal. Background technique [0002] Polyoxymethylene dimethyl ether (Chinese name can also be polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, polyoxymethylene dimethyl ether, etc.), that is, polyoxymethylene dimethyl ethers ( PODE), it is a general term for a class of substances, its molecular structure is CH 3 O(CH 2 O) n CH 3 , with higher cetane number (cetane number, CN. When n=3~8, CN>76) and oxygen content (42~49%). When the value of n is 3 to 8, its physical and chemical properties and combustion performance are very close to those of diesel oil, and it can be used as a diesel oil additive. The amount added to diesel oil can reach 30% (v / v), while maintaining a high ten Hexane number and combustion performance. It can improve the lubricity of diesel, reduce the generation of combustion smoke, improve the combustion status of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/303C07C41/56C08G2/08C08G2/10C08G2/06B01J29/40B01J35/10
CPCY02P20/52
Inventor 何欣刘志成高焕新
Owner CHINA PETROLEUM & CHEM CORP
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